Sodium Hydroxide → Cimlanod

HRID 1749192ノート

反応式

HRID 1749192 の反応式
C[C@H]1[O:7][C@@H]2O[C@H]3[C@H](O)[C@@H](O)[C@@H](O[C@H]4[C@H](O)[C@@H](O)[C@@H](O[C@H]5[C@H](O)[C@@H](O)[C@@H](O[C@H]6[C@H](O)[C@@H](O)[C@@H](O[C@H]7[C@H](O)[C@@H](O)[C@@H](O[C@H]8[C@H](O)[C@@H](O)[C@@H](O[C@H]1[C@H](O)[C@H]2O)O[C@@H]8COCCCCS([O-])(=O)=O)O[C@@H]7CO)O[C@@H]6CO)O[C@@H]5CO)O[C@@H]4CO)O[C@@H]3CO.[Na+].[OH-].[Na+].[OH:88][NH:89][S:90]([C:93]1C=[CH:97][CH:96]=[C:95](S(C)(=O)=O)[CH:94]=1)(=[O:92])=[O:91]>O>[OH:88][NH:89][S:90]([C:93]1[O:7][C:96]([CH3:97])=[CH:95][CH:94]=1)(=[O:92])=[O:91]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 76901580N-Hydroxy-3-methanesulfonylbenzene-1-sulfonamide2 回HCID 91886200Sulfobutylether--Cyclodextrin

生成物 1

HCID 76685198Cimlanod

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Additionally, a sample of the compound of formula (1) was prepared in water to determine the approximate solubility of the compound in the absence of excipients (e.g., CAPTISOL®). A concentration of approximately 300 mg/mL was achieved, not accounting for the volume contribution of the compound. The pH of the sample was determined to be 2.8, which was adjusted to the target of 4.0 using 0.1 N NaOH. Upon pH adjustment, precipitation of a small amount of solid was observed. The clear solution was diluted in acetonitrile and analyzed by HPLC, resulting in an observed solution concentration of 268 mg/mL. A similar analysis was performed for the compound of formula (2). The compound of formula (2) has a solubility of approximately 10 mg/mL.

後処理

  1. customUpon pH adjustment, precipitation of a small amount of solid
  2. additionThe clear solution was diluted in acetonitrile
  3. customresulting in an observed solution concentration of 268 mg/mL

出典と根拠

ORDレコード
ord-22b42041d4d4440999f071e4d419c272
出典データセット
uspto-grants-2015_10
特許番号
US09156804B2

反応ノート

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